Methanesulfonyl chloride → N-(2-Fluoro-4-hydroxyphenyl)methanesulfonamide

HRID 133782노트

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HRID 133782 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][C:3]=1[F:9].[CH3:10][S:11](Cl)(=[O:13])=[O:12]>N1C=CC=CC=1>[F:9][C:3]1[CH:4]=[C:5]([OH:8])[CH:6]=[CH:7][C:2]=1[NH:1][S:11]([CH3:10])(=[O:13])=[O:12]

참가 물질

4

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 27359194-Amino-3-fluorophenol

생성물 1

HCID 64786305N-(2-Fluoro-4-hydroxyphenyl)methanesulfonamide

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
0 °C

실험 절차

4-Amino-3-fluorophenol (0.254 g; 2.0 mmol) was dissolved in 10 ml of dry pyridine under nitrogen and cooled to 0° C. Methanesulfonyl chloride (0.17 ml; 2.1 mmol) was added dropwise and stirred for three days at room temperature. The reaction was evaporated, 25 ml of toluene added and evaporated again. Toluene evaporation was repeated. Residue was dissolved in 25 ml of EtOAc, washed with 20 ml of water and evaporated to dryness to give red-brown solid N-(2-fluoro-4-hydroxyphenyl)methanesulfonamide. 1H NMR (400 MHz, DMSO-d6): 2.93 (3H, s), 6.56-6.66 (2H, m), 7.14 (1H, t, J=9.0 Hz), 9.17 (1H, s), 9.98 (1H, s).

후처리

  1. customThe reaction was evaporated
  2. addition25 ml of toluene added
  3. customevaporated again
  4. customToluene evaporation
  5. dissolutionResidue was dissolved in 25 ml of EtOAc
  6. washwashed with 20 ml of water
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-ba401eddf8cd49a1b705a09f6d86b330
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07390923B2

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